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The rational modulation of metal catalysts with tailorable valence and redox properties is a promising strategy for further improving their catalytic performance. Herein, an environment-friendly grafting and thermal strategy was adopted to immobilize copper oxides nanoparticles on carbon nanofiber (CuOx/CF). Benefiting from the defect-rich surface and valence-mixed composition of the CuOx species, the optimized sample CuOx/CF-3 exhibits superb activity for the catalytic reduction of toxic nitrophenols. The complete conversion took only 1 min and an outstanding rate constant (k) of 112.7 × 10-3 s-1 was achieved under mild conditions (25 °C and 1 atm). Kinetic and recycle experiments demonstrated that the whole catalytic process obeys a pseudo-order kinetic, and the catalyst could maintain high conversion even after 13 successive recycles. These results demonstrate that CuOx/CF-3 is an alternative catalyst to noble metals, providing superb catalytic efficiency and stability in the reduction of toxic nitrophenols, and it can be expanded to develop other noble-metal-free catalysts for various applications.